该文建立了顶空气相色谱法测定酒中氰化物含量的方法.酒样品用氯胺T将氰化物衍生为氯化氰,顶空进样,经WAX气相色谱柱(30 m×0.32 mm×0.50μm)分离,电子捕获检测器(ECD)检测,外标法定量.同时对检测过程中的衍生剂用量、衍生酸度、顶空平衡温度、顶空平衡时间、气相色谱条件进行优化,结果表明:氰离子在0.001 mg/L~0.1 mg/L范围内线性良好,相关系数可达到0.998,定量限(以信噪比(S/N)≥10)为0.05 mg/L.在0.1、0.2、8.0 mg/L 3个添加水平下进行了回收率和精密度试验,其中加标回收率在84.1%~109.7%之间,相对标准偏差RSD(n=10)为4.41%~6.54%,满足日常的检测要求.与传统的分光光度法相比,该方法操作简便、快速、稳定性好、灵敏度高、抗干扰能力强,在实际工作中有很好的应用价值.%A method for determination of cyanide residue in wine by headspace gas chromatography was de-scribed.Win added chloramine T to make cyanide derivative as cyanogen chloride, head-space injection, then separated it by the WAX gas chromatographic column, detected by electron capture detector ECD and quanti-fied by external standard. The results showed as follow, the linear range was 0.001 mg/L-0.1 mg/L,the correla-tion coefficient was 0.998 and the limit of detection(S/N≥10)was 0.05 mg/L. Recoveries were 4.41%-6.54%with RSD (n=10) at the three different standards levels of 0.1,0.2,8.0 mg/L. The method is simple, rapid, ac-curate, and can be applied in the determination of cyanide in vinic products,and meet requirements of the daily testing. Meanwhile, the dosage of the derivative, headspace holding time and the temperature were optimized.
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